CN108948972A - The preparation method of multi-functional dumb light resin and its application in paint of coating - Google Patents

The preparation method of multi-functional dumb light resin and its application in paint of coating Download PDF

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Publication number
CN108948972A
CN108948972A CN201810766753.1A CN201810766753A CN108948972A CN 108948972 A CN108948972 A CN 108948972A CN 201810766753 A CN201810766753 A CN 201810766753A CN 108948972 A CN108948972 A CN 108948972A
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parts
resin
dumb light
white carbon
functional
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宣全
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Quechen Silicon Chemical Co Ltd
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宣全
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
    • C09D163/10—Epoxy resins modified by unsaturated compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/42—Gloss-reducing agents
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/32—Phosphorus-containing compounds
    • C08K2003/321—Phosphates
    • C08K2003/324—Alkali metal phosphate
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend

Abstract

The present invention relates to the preparation method of multi-functional dumb light resin and its applications in paint of coating, the formula is grouped as by the group of following parts by weight: 60-80 parts of resin, 10-30 parts of delustering agent, 2-3 parts of dispersing agent, 20-40 parts of butyl ester, wherein delustering agent is made of 2-8 parts of 5-16 parts of wax emulsions of parts by weight, 3-6 parts of metallic soaps of parts by weight, parts by weight modified white carbon blacks.Dumb light resin hardness scratch resistant effect of the invention is obvious, and flatting efficiency is high, applied widely, and cost performance is high；Dust yield can be effectively reduced, operating procedure is simply time saving and energy saving；Transparency improves 20%-30%, and resistance to Huang effect improves 10%-25%, brushes area and improve 2%-5%.

Description

The preparation method of multi-functional dumb light resin and its application in paint of coating
Technical field
The present invention relates to woodcare paint class coating, a kind of preparation method more particularly to multi-functional dumb light resin and its are applying Application in material.
Background technique
Woodwork coating has critical role and effect in wood-processing industry.The woodwork coating that the country uses at present is mainly Solvent based coating, containing a large amount of organic volatiles (VOC), part coatings contain the height carcinogenicity object such as benzene,toluene,xylene Matter seriously affects indoor air quality and the health of the mankind.
Common low luster coating is mostly to be deployed with flatting silica currently on the market, main body be hydroxyl polyester resin, Acrylic resin and polyurethane curing agent system or thermoplastic propene's acid system are formed added with machine pigment, auxiliary agent and solvent, this In actual application, application property is difficult to control coating, and same bucket paint in construction, waved using difference by different film thickness The diluent gloss for sending out speed is widely different, and the problems such as floating often occurs in the arrangement of flatting silica；Construct solid content it is low, VOC emission amount is high, can not meet the requirement of environmental protection.With dumb light resin allotment dumb light paint on the market, cost superelevation, and roller coating Matte effect is poor；The dumb light resin of domestic rare autonomous synthesis, allotment.Currently, skill existing for the low luster coating of flatting silica allotment Art problem is:
1, construction solid content is low, VOC discharge amount is high；
2, application property is poor, unstable；
3, controlling of production process is complicated.
The paint film of woodcare paint is soft, temperature-change resistance is poor, wear-resisting, film forming speed is slow, and nano material has very high specific surface area, A variety of secondary valences can be formed with the chain in organic polymer and are good for binding force, and under stress, this binding force can be destroyed, and be made Macromolecular chain is locally slipped from Nanosurface;Simultaneously this active force can re-form again, make polymer chain slippage part or Other part is recombined with nano material, so that being not easy to be destroyed in stress.
A kind of dumb light resin and preparation method thereof is disclosed in Chinese patent literature " (104231892 A of CN) ", this is matched Side is grouped as by the group of following parts by weight: 60-70 parts of medium oil alkyd；3-5 parts of acetylbutyrylcellulose；Polyamide 2-5 parts of wax；4-8 parts of SCA modified polyester resin；8-15 parts of ethylene-vinyl acetate copolymer wax dispenser；Rheology control Auxiliary agent 0.1-1 parts processed；3-10 parts of dimethylbenzene；3-5 parts of butyl acetate.Obtained dumb light resin flexible good toughness, it is resistance to 140-170 DEG C of high-temperature baking, can be machined out smart car, and gloss stability is good.
Summary of the invention
The object of the present invention is to provide a kind of multi-functional dumb light resins, to overcome existing for existing flatting silica low luster coating The problem that VOC emission amount is high, transparency is not high；Richness, the hardness, transparency of multi-functional dumb light resin are improved simultaneously, and wide It is general to be suitable for all kinds of coating modes.The present invention is achieved by the following technical solutions:
A kind of multi-functional dumb light resin, which is characterized in that be grouped as by the group of following parts by weight: 60-80 parts of resin, delustering agent 10-30 parts, 2-5 parts of dispersing agent, 20-40 parts of butyl ester, wherein delustering agent is by 3-6 parts of 5-16 parts of wax emulsions of parts by weight, parts by weight gold Belong to 2-8 parts of soap, parts by weight modified white carbon black compositions.
In a preferred embodiment of invention, raw material white carbon black used in the modified white carbon black is fumed silica M-5, modified white carbon black purity are 99.5-99.8%, specific surface area are as follows: 110-150m2/ g, partial size are as follows: 7-40nm.
In a preferred embodiment of invention, the wax emulsion is aqueous polyethylene wax emulsion.
In a preferred embodiment of invention, the metallic soap is in zinc stearate, calcium stearate or odium stearate One or more.
In a preferred embodiment of invention, the dispersing agent is BH616, DP983, BYKP-105 and Disper710 At least one of dispersing agent.
In a preferred embodiment of invention, the resin is modified polyacrylate resin, is epoxy group acrylic acid The mixture of resin and Hydroxylated acrylic resin, mass ratio 1:1.
The preparation method of a kind of multi-functional dumb light resin, which is characterized in that the preparation method of modified white carbon black is such as Under:
1. white carbon black is crushed, it is sieved, obtains sieving, sieving is mixed with liquor potassic permanganate, immersion 1 ~ 2h, filtering, obtains filter residue, filter residue is washed with water and is dried at 100 ~ 120 DEG C of temperature, fine powder is ground into after drying；
1. score meter by weight crushes 100 parts of white carbon blacks, sieving obtains sieving, and sieving is molten with sodium tripolyphosphate Liquid, 200-300 part are mixed, and 1 ~ 2h is impregnated, and filtering obtains filter residue, filter residue washed with ferroso-ferric oxide, in temperature 100 It is dried at ~ 120 DEG C, fine powder is ground into after drying；
2. taking 3-10 parts of mutual-amido two polyaniline, 3-10 parts of nylon powder, 10-30 parts of initiator, 10-30 parts of addition reactions of polyethylene glycol Kettle is mixed, magnetic agitation 1h；
3. reaction kettle, which is added, in white carbon black obtains mixture, 99% nitrogen is injected, keeping the pressure of reaction kettle is 2.1Kg/cm2, temperature It is 1400 DEG C, reacts 120 minutes, resulting material out is put into a centrifuge and is centrifuged, centrifugation object is obtained；
4. by step, 3. for resulting centrifugation object through ultrasonic wave and microwave combined processing, ultrasonic technology parameter is frequency 20- 100KHz, 100-2000 watts of power；Microwave technology parameters frequency be 880-2500MHz, 300-1500 watts of power, Combined Treatment Time be 10-150 minute, control temperature at 50-70 DEG C；
5. by step, 4. resulting product is mixed with 30-50 parts of titanate coupling agents at a temperature of 30-60 DEG C and is coupled, later Refilter, wash, 600-900 DEG C calcining 2-6 hours, obtain described in modified white carbon black.
The preparation method of dumb light resin of the invention the following steps are included:
1. the preparation of delustering agent: after wax emulsion is mixed evenly with metallic soap, the table of white carbon black is sprayed in spraying form Face is simultaneously mixed, and obtains 0.5-3 microns of partial size, pH value is between 6.5-7.5；
2. at room temperature, the delustering agent by step (1) preparation is added in separating apparatus, revolving speed is adjusted to 400r/min, stirring Under, resin is added, revolving speed is adjusted to 1200r/min, after high speed dispersion 30min, it is stand-by to obtain homogeneous viscous fluid A；
3. being slowly added in dispersing agent under stirring, revolving speed is adjusted to 800r/min, 30min is stirred, obtains homogeneous solution B；
4. being slowly added to butyl ester in separating apparatus, revolving speed is adjusted to 400r/min, it is resulting that step (3) are added under stirring Even liquid B, is adjusted to 1200r/min for mixing speed after the completion of charging, continues to stir 20min, after test traditional performance is qualified, i.e., Dumb light resin is made.
In a preferred embodiment of invention, initiator is hydroperoxides, dialkyl, diacyl peroxides times It anticipates one kind.
In a preferred embodiment of invention, multi-functional dumb light resin is in 5-40 parts of addition paint of coating with parts by weight.
After above-mentioned technical solution, the beneficial effect that the present invention obtains is: dumb light resin hardness scratch resistant effect is bright Aobvious, flatting efficiency is high, applied widely, and cost performance is high；Dust yield can be effectively reduced, operating procedure is simply time saving and energy saving； Transparency improves 20%-30%, and resistance to Huang effect improves 10%-25%, brushes area and improve 2%-5%.
Specific embodiment
Form by the following examples is described in further detail above content of the invention again, but should not be by this The range for being interpreted as the above-mentioned theme of the present invention is only limitted to following embodiment, all technologies based on realization belonging to above content of the present invention It all belongs to the scope of the present invention.
Specific targets testing standard:
Coating Voc content detection made from multi-functional dumb light resin is measured by GB 18582-2001；Yellowing resistance is investigated The case where ginkgo seeds turn to be yellow under action of ultraviolet light is tested by IOS-MAT-0050 method, by standard GB/T/T1766-1995 Regulation carries out；Solid content can quantitatively determine film forming matter content in aqueous woodware paint, and the measurement of solid content uses GB/ Tl725-2007；GB/T9754-88 is pressed in the measurement of coating gloss made from multi-functional dumb light resin；GB/ is pressed in the measurement of fineness Tl724-1979(1989 it) is measured；The viscosity method of inspection is measured using rotational viscometer method in GB/T1723-1993； The transparency of dumb light cold coating is detected according to GB/T1721-2008 method.
Embodiment 1:
Resin formula are as follows:
It is grouped as by the group of following parts by weight: 60 parts of resin, 30 parts of delustering agent, 2 parts of dispersing agent, 20-40 parts of butyl ester.Delustering agent It is made of 8 parts of 16 parts of wax emulsions, 6 parts of metallic soaps of parts by weight, parts by weight modified white carbon blacks.Modified white carbon black purity is 99.8%, Modified white carbon black specific surface area are as follows: 150m2/g；The partial size of modified white carbon black are as follows: 20nm；The wax emulsion is aqueous polyethylene Wax emulsion；The metallic soap is zinc stearate；The dispersing agent is BH616；The resin be epoxy group acrylic resin with The mass ratio of the mixture of Hydroxylated acrylic resin, epoxy group acrylic resin and Hydroxylated acrylic resin is 1:1.
The preparation of modified white carbon black:
1. score meter by weight crushes 100 parts of white carbon blacks, sieving obtains sieving, and sieving is molten with sodium tripolyphosphate 300 parts of liquid are mixed, and 2h is impregnated, and filtering obtains filter residue, filter residue is washed with ferroso-ferric oxide, dries at 120 DEG C of temperature, Fine powder is ground into after drying；
2. taking 10 parts of mutual-amido two polyaniline, 10 parts of nylon powder, 10 parts of initiator, 10 parts of addition reaction kettles of polyethylene glycol are mixed It closes, magnetic agitation 1h；
3. reaction kettle, which is added, in white carbon black obtains mixture, 99% nitrogen is injected, keeping the pressure of reaction kettle is 2.1Kg/cm2, temperature It is 1400 DEG C, reacts 120 minutes, resulting material out is put into a centrifuge and is centrifuged, centrifugation object is obtained；
4. by step, 3. for resulting centrifugation object through ultrasonic wave and microwave combined processing, ultrasonic technology parameter is frequency 100KHz, 2000 watts of power；Microwave technology parameters frequency is 2500MHz, and 1500 watts of power, the time of Combined Treatment is 30 minutes, control temperature Degree is at 50 DEG C；
5. by step, 4. resulting product is mixed with 50 parts of titanate coupling agents at a temperature of 30 DEG C and is coupled, later after Filter, washing are calcined 2 hours at 600 DEG C, obtain the modified white carbon black.
The preparation of resin:
1. the preparation of delustering agent: after wax emulsion is mixed evenly with metallic soap, being sprayed at modified white carbon black in spraying form Surface and mixed；
2. the delustering agent at room temperature, 1. step prepared is added in separating apparatus, revolving speed is adjusted to 400r/min, stirring Under, resin is added, revolving speed is adjusted to 1200r/min, after high speed dispersion 30min, it is stand-by to obtain homogeneous viscous fluid A；
3. being slowly added in dispersing agent under stirring, revolving speed is adjusted to 800r/min, 30min is stirred, obtains homogeneous solution B；
4. being slowly added to butyl ester in separating apparatus, revolving speed is adjusted to 400r/min, it is resulting that step (3) are added under stirring Even liquid B, is adjusted to 1200r/min for mixing speed after the completion of charging, continues to stir 20min, after test traditional performance is qualified, i.e., Dumb light resin is made.
The initiator is hydroperoxides；Multi-functional dumb light resin is in 10 parts of addition paint of coating with parts by weight.
To prepare the viscosity in multi-functional dumb light cold coating sample, fineness, VOC content, solid content, acid value, hydroxyl value, Resistance to Huang effect, gloss are tested, and the transparency of multi-functional dumb light cold coating is examined according to GB/T1721-2008 method It surveys.
Embodiment 2:
Resin formula are as follows:
It is grouped as by the group of following parts by weight: 80 parts of resin, 15 parts of delustering agent, 2-3 parts of dispersing agent, 20-40 parts of butyl ester.Delustring Agent is made of 5 parts of 5 parts of wax emulsions, 3 parts of metallic soaps of parts by weight, parts by weight modified white carbon blacks.White carbon black purity is 99.5- 99.8%, white carbon black specific surface area are as follows: 110-150m2/g；The partial size of white carbon black are as follows: 7-40nm；The wax emulsion is aqueous poly- Ethylene wax emulsion.The metallic soap is calcium stearate；The dispersing agent is DP983；The resin is epoxy group acrylic acid tree The mass ratio of the mixture of rouge and Hydroxylated acrylic resin, epoxy group acrylic resin and Hydroxylated acrylic resin is 1:1.
The preparation of modified white carbon black:
1. score meter by weight crushes 100 parts of white carbon blacks, sieving obtains sieving, and sieving is molten with sodium tripolyphosphate 300 parts of liquid are mixed, and 2h is impregnated, and filtering obtains filter residue, filter residue is washed with ferroso-ferric oxide, dries at 120 DEG C of temperature, Fine powder is ground into after drying；
2. taking 3 parts of mutual-amido two polyaniline, 3 parts of nylon powder, 10 parts of initiator, 10 parts of addition reaction kettles of polyethylene glycol are mixed, Magnetic agitation 1h；
3. reaction kettle, which is added, in white carbon black obtains mixture, 99% nitrogen is injected, keeping the pressure of reaction kettle is 2.1Kg/cm2, temperature It is 1400 DEG C, reacts 120 minutes, resulting material out is put into a centrifuge and is centrifuged, centrifugation object is obtained；
4. by step, 3. for resulting centrifugation object through ultrasonic wave and microwave combined processing, ultrasonic technology parameter is frequency 20- 100KHz, 100-2000 watts of power；Microwave technology parameters frequency be 880-2500MHz, 300-1500 watts of power, Combined Treatment Time be 50 minutes, control temperature at 50-70 DEG C；
5. by step, 4. resulting product mixes with 30 parts of titanate coupling agents be coupled at 50 °C, later after Filter, washing are calcined 3 hours at 900 DEG C, obtain the modified white carbon black.
The preparation of resin:
1. the preparation of delustering agent: after wax emulsion is mixed evenly with metallic soap, the table of white carbon black is sprayed in spraying form Face is simultaneously mixed；
2. at room temperature, the delustering agent by step (1) preparation is added in separating apparatus, revolving speed is adjusted to 400r/min, stirring Under, resin is added, revolving speed is adjusted to 1200r/min, after high speed dispersion 30min, it is stand-by to obtain homogeneous viscous fluid A；
3. being slowly added in dispersing agent under stirring, revolving speed is adjusted to 800r/min, 30min is stirred, obtains homogeneous solution B；
4. being slowly added to butyl ester in separating apparatus, revolving speed is adjusted to 400r/min, it is resulting that step (3) are added under stirring Even liquid B, is adjusted to 1200r/min for mixing speed after the completion of charging, continues to stir 20min, after test traditional performance is qualified, i.e., Dumb light resin is made.
Initiator is diacyl peroxides, and multi-functional dumb light resin is in 30 parts of addition paint of coating with parts by weight.
To prepare the viscosity in multi-functional dumb light cold coating sample, fineness, VOC content, solid content, acid value, hydroxyl value, Resistance to Huang effect, gloss are tested, and the transparency of multi-functional dumb light cold coating is examined according to GB/T1721-2008 method It surveys；The results are shown in Table 1.
Embodiment 3:
Resin formula are as follows:
It is grouped as by the group of following parts by weight: 80 parts of resin, 20 parts of delustering agent, 3 parts of dispersing agent, 40 parts of butyl ester.Delustering agent is by 10 5 parts of part wax emulsion, 5 parts of metallic soaps of parts by weight, parts by weight modified white carbon blacks compositions.White carbon black purity is 99.5-99.8%, hard charcoal Black specific surface area are as follows: 110-150m2/g；The partial size of white carbon black are as follows: 7-40nm, the wax emulsion are aqueous polyethylene wax cream Liquid；The metallic soap is odium stearate；Dispersing agent is BYKP-105；The resin is epoxy group acrylic resin and hydroxyl third The mass ratio of the mixture of olefin(e) acid resin, epoxy group acrylic resin and Hydroxylated acrylic resin is 1:1.
The preparation of modified white carbon black:
1. score meter by weight crushes 100 parts of white carbon blacks, sieving obtains sieving, and sieving is molten with sodium tripolyphosphate 200 parts of liquid are mixed, and 2h is impregnated, and filtering obtains filter residue, filter residue is washed with ferroso-ferric oxide, dries at 100 DEG C of temperature, Fine powder is ground into after drying；
2. taking 8 parts of mutual-amido two polyaniline, 8 parts of nylon powder, 20 parts of initiator, 20 parts of addition reaction kettles of polyethylene glycol are mixed, Magnetic agitation 1h；
3. reaction kettle, which is added, in white carbon black obtains mixture, 99% nitrogen is injected, keeping the pressure of reaction kettle is 2.1Kg/cm2, temperature It is 1400 DEG C, reacts 120 minutes, resulting material out is put into a centrifuge and is centrifuged, centrifugation object is obtained；
4. by step, 3. for resulting centrifugation object through ultrasonic wave and microwave combined processing, ultrasonic technology parameter is frequency 20KHz, function 100 watts of rate；Microwave technology parameters frequency is 2500MHz, and 1500 watts of power, the time of Combined Treatment is 150 minutes, control temperature Degree is at 50 DEG C；
5. by step, 4. resulting product is mixed with 40 parts of titanate coupling agents at a temperature of 60 DEG C and is coupled, later after Filter, washing are calcined 6 hours at 600 DEG C, obtain the modified white carbon black.
The preparation of resin:
1. the preparation of delustering agent: after wax emulsion is mixed evenly with metallic soap, the table of white carbon black is sprayed in spraying form Face is simultaneously mixed；
2. at room temperature, the delustering agent by step (1) preparation is added in separating apparatus, revolving speed is adjusted to 400r/min, stirring Under, resin is added, revolving speed is adjusted to 1200r/min, after high speed dispersion 30min, it is stand-by to obtain homogeneous viscous fluid A；
3. being slowly added in dispersing agent under stirring, revolving speed is adjusted to 800r/min, 30min is stirred, obtains homogeneous solution B；
4. being slowly added to butyl ester in separating apparatus, revolving speed is adjusted to 400r/min, it is resulting that step (3) are added under stirring Even liquid B, is adjusted to 1200r/min for mixing speed after the completion of charging, continues to stir 20min, after test traditional performance is qualified, i.e., Dumb light resin is made.
Initiator is diacyl peroxides；Multi-functional dumb light resin is in 26 parts of addition paint of coating with parts by weight.
To prepare the viscosity in multi-functional dumb light cold coating sample, fineness, VOC content, solid content, acid value, hydroxyl value, Resistance to Huang effect, gloss are tested, and the transparency of multi-functional dumb light cold coating is examined according to GB/T1721-2008 method It surveys.
Embodiment 4:
Resin formula are as follows:
It is grouped as by the group of following parts by weight: 80 parts of resin, 30 parts of delustering agent, 2 parts of dispersing agent, 40 parts of butyl ester.Delustering agent is by 16 8 parts of part wax emulsion, 6 parts of metallic soaps of parts by weight, parts by weight modified white carbon blacks compositions.White carbon black purity is 99.8%, white carbon black ratio Surface area are as follows: 150m2/g；The partial size of white carbon black are as follows: 7nm；
The wax emulsion is aqueous polyethylene wax emulsion；The metallic soap is zinc stearate；The dispersing agent is Disper710；The resin is the mixture of epoxy group acrylic resin and Hydroxylated acrylic resin, epoxy group acrylic resin Mass ratio with Hydroxylated acrylic resin is 1:1；
The preparation of modified white carbon black:
1. score meter by weight crushes 100 parts of white carbon blacks, sieving obtains sieving, and sieving is molten with sodium tripolyphosphate Liquid, 300 parts mixed, impregnate 2h, filtering, obtain filter residue, filter residue washed with ferroso-ferric oxide, dried at 120 DEG C of temperature, Fine powder is ground into after drying；
2. taking 7 parts of mutual-amido two polyaniline, 7 parts of nylon powder, 30 parts of initiator, 30 parts of addition reaction kettles of polyethylene glycol are mixed, Magnetic agitation 1h；
3. reaction kettle, which is added, in white carbon black obtains mixture, 99% nitrogen is injected, keeping the pressure of reaction kettle is 2.1Kg/cm2, temperature It is 1400 DEG C, reacts 120 minutes, resulting material out is put into a centrifuge and is centrifuged, centrifugation object is obtained；
4. by step, 3. for resulting centrifugation object through ultrasonic wave and microwave combined processing, ultrasonic technology parameter is frequency 50KHz, function 1000 watts of rate；Microwave technology parameters frequency is 1000MHz, and 1000 watts of power, the time of Combined Treatment is 30 minutes, control temperature Degree is at 70 DEG C；
5. by step, 4. resulting product is mixed with 30 parts of titanate coupling agents at a temperature of 60 DEG C and is coupled, later after Filter, washing are calcined 6 hours at 900 DEG C, obtain the modified white carbon black.
The preparation of resin:
1. the preparation of delustering agent: after wax emulsion is mixed evenly with metallic soap, the table of white carbon black is sprayed in spraying form Face is simultaneously mixed, and obtains 3 microns of partial size, pH value is between 7.5；
2. at room temperature, the delustering agent by step (1) preparation is added in separating apparatus, revolving speed is adjusted to 400r/min, stirring Under, resin is added, revolving speed is adjusted to 1200r/min, after high speed dispersion 30min, it is stand-by to obtain homogeneous viscous fluid A；
3. being slowly added in dispersing agent under stirring, revolving speed is adjusted to 800r/min, 30min is stirred, obtains homogeneous solution B；
4. being slowly added to butyl ester in separating apparatus, revolving speed is adjusted to 400r/min, it is resulting that step (3) are added under stirring Even liquid B, is adjusted to 1200r/min for mixing speed after the completion of charging, continues to stir 20min, after test traditional performance is qualified, i.e., Dumb light resin is made.
Initiator is hydroperoxides；Multi-functional dumb light resin is in 26 parts of addition paint of coating with parts by weight.
To prepare the viscosity in multi-functional dumb light cold coating sample, fineness, VOC content, solid content, acid value, hydroxyl value, Resistance to Huang effect, gloss are tested, and the transparency of multi-functional dumb light cold coating is examined according to GB/T1721-2008 method It surveys.
Comparative example 1:
Resin formula are as follows:
It is grouped as by the group of following parts by weight: 50 parts of resin, 5 parts of delustering agent, 6 parts of dispersing agent, 30 parts of butyl ester.Delustering agent is by 4 parts 5 parts of wax emulsion, 3 parts of metallic soaps of parts by weight, parts by weight modified white carbon black compositions.White carbon black purity is 99.5%, and white carbon black compares table Area are as follows: 150m2/g；The partial size of white carbon black are as follows: 50nm.
The preparation of modified white carbon black:
1. score meter by weight crushes 100 parts of white carbon blacks, sieving obtains sieving, and sieving is molten with sodium tripolyphosphate Liquid, 300 parts mixed, impregnate 2h, filtering, obtain filter residue, filter residue washed with ferroso-ferric oxide, dried at 120 DEG C of temperature It is dry, fine powder is ground into after drying；
2. taking 2 parts of mutual-amido two polyaniline, 2 parts of nylon powder, 40 parts of initiator, 30 parts of addition reaction kettles of polyethylene glycol are mixed, Magnetic agitation 1h；
3. reaction kettle, which is added, in white carbon black obtains mixture, 99% nitrogen is injected, keeping the pressure of reaction kettle is 2.1Kg/cm2, temperature It is 1400 DEG C, reacts 120 minutes, resulting material out is put into a centrifuge and is centrifuged, centrifugation object is obtained；
4. by step, 3. for resulting centrifugation object through ultrasonic wave and microwave combined processing, ultrasonic technology parameter is frequency 100KHz, 2000 watts of power；Microwave technology parameters frequency is 2500MHz, and 1500 watts of power, the time of Combined Treatment is 10 minutes, control Temperature is at 70 DEG C；
5. by step, 4. resulting product is mixed with 50 parts of titanate coupling agents at a temperature of 30 DEG C and is coupled, later after Filter, washing are calcined 2 hours at 600 DEG C, obtain the modified white carbon black.
The preparation of resin:
1. the preparation of delustering agent: after wax emulsion is mixed evenly with metallic soap, the table of white carbon black is sprayed in spraying form Face is simultaneously mixed, and obtains 0.5 micron of partial size, pH value is between 7.5；
2. at room temperature, the delustering agent by step (1) preparation is added in separating apparatus, revolving speed is adjusted to 400r/min, stirring Under, resin is added, revolving speed is adjusted to 1200r/min, after high speed dispersion 30min, it is stand-by to obtain homogeneous viscous fluid A；
3. being slowly added in dispersing agent under stirring, revolving speed is adjusted to 800r/min, 30min is stirred, obtains homogeneous solution B；
4. being slowly added to butyl ester in separating apparatus, revolving speed is adjusted to 400r/min, it is resulting that step (3) are added under stirring Even liquid B, is adjusted to 1200r/min for mixing speed after the completion of charging, continues to stir 20min, after test traditional performance is qualified, i.e., Dumb light resin is made.
Initiator is hydroperoxides；Multi-functional dumb light resin is in 2 parts of addition paint of coating with parts by weight.
To prepare the viscosity in multi-functional dumb light cold coating sample, fineness, VOC content, solid content, acid value, hydroxyl value, Resistance to Huang effect, gloss are tested, and the transparency of multi-functional dumb light cold coating is examined according to GB/T1721-2008 method It surveys.
Comparative example 2: using not modified white carbon black, steps are as follows；
Resin formula are as follows: be grouped as by the group of following parts by weight: 80 parts of resin, 30 parts of delustering agent, 2 parts of dispersing agent, butyl ester 40 Part.Delustering agent is made of 8 parts of 16 parts of wax emulsions, 6 parts of metallic soaps of parts by weight, parts by weight white carbon blacks；The wax emulsion is aqueous Polythene wax emulsion；The metallic soap is zinc stearate；The dispersing agent is Disper710；The resin is epoxy group third The mass ratio of the mixture of olefin(e) acid resin and Hydroxylated acrylic resin, epoxy group acrylic resin and Hydroxylated acrylic resin is 1: 1；
The preparation of resin:
1. the preparation of delustering agent: after wax emulsion is mixed evenly with metallic soap, the table of white carbon black is sprayed in spraying form Face is simultaneously mixed, and obtains 3 microns of partial size, pH value is between 7.5；
2. at room temperature, the delustering agent by step (1) preparation is added in separating apparatus, revolving speed is adjusted to 400r/min, stirring Under, resin is added, revolving speed is adjusted to 1200r/min, after high speed dispersion 30min, it is stand-by to obtain homogeneous viscous fluid A；
3. being slowly added in dispersing agent under stirring, revolving speed is adjusted to 800r/min, 30min is stirred, obtains homogeneous solution B；
4. being slowly added to butyl ester in separating apparatus, revolving speed is adjusted to 400r/min, it is resulting that step (3) are added under stirring Even liquid B, is adjusted to 1200r/min for mixing speed after the completion of charging, continues to stir 20min, after test traditional performance is qualified, i.e., Dumb light resin is made.
To prepare the viscosity in multi-functional dumb light cold coating sample, fineness, VOC content, solid content, acid value, hydroxyl value, Resistance to Huang effect, gloss are tested, and the transparency of multi-functional dumb light cold coating is examined according to GB/T1721-2008 method It surveys.
Comparative example 3: being not added white carbon black in resin formula, steps are as follows；
Resin formula are as follows:
It is grouped as by the group of following parts by weight: 80 parts of resin, 30 parts of delustering agent, 2 parts of dispersing agent, 40 parts of butyl ester.Delustering agent is by 16 Part 6 parts of wax emulsion, parts by weight metallic soaps.The wax emulsion is aqueous polyethylene wax emulsion；The metallic soap is zinc stearate； The dispersing agent is Disper710；The resin is the mixture of epoxy group acrylic resin and Hydroxylated acrylic resin, The mass ratio of epoxy group acrylic resin and Hydroxylated acrylic resin is 1:1.
The preparation of resin:
1. the preparation of delustering agent: after wax emulsion is mixed evenly with metallic soap, the table of white carbon black is sprayed in spraying form Face is simultaneously mixed, and obtains 3 microns of partial size, pH value is between 7.5；
2. at room temperature, the delustering agent by step (1) preparation is added in separating apparatus, revolving speed is adjusted to 400r/min, stirring Under, resin is added, revolving speed is adjusted to 1200r/min, after high speed dispersion 30min, it is stand-by to obtain homogeneous viscous fluid A；
3. being slowly added in dispersing agent under stirring, revolving speed is adjusted to 800r/min, 30min is stirred, obtains homogeneous solution B；
4. being slowly added to butyl ester in separating apparatus, revolving speed is adjusted to 400r/min, it is resulting that step (3) are added under stirring Even liquid B, is adjusted to 1200r/min for mixing speed after the completion of charging, continues to stir 20min, after test traditional performance is qualified, i.e., Dumb light resin is made；Multi-functional dumb light resin is in 20 parts of addition paint of coating with parts by weight.
To prepare the viscosity in multi-functional dumb light cold coating sample, fineness, VOC content, solid content, acid value, hydroxyl value, Resistance to Huang effect, gloss are tested, and the transparency of multi-functional dumb light cold coating is examined according to GB/T1721-2008 method It surveys.
Comparative example 4
The dumb light resin referring to made from the method in 104231892 A of patent CN.
To prepare the viscosity in multi-functional dumb light cold coating sample, fineness, VOC content, solid content, acid value, hydroxyl value, Resistance to Huang effect, gloss are tested, and the transparency of multi-functional dumb light cold coating is examined according to GB/T1721-2008 method It surveys.
Table 1
Project Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4 Comparative example 1 Comparative example 2 Comparative example 3 Comparative example 4
Viscosity (mpa s/25 DEG C) 31800 30000 30900 27090 30000 27600 20000 38000
Fineness μm 10 10.5 12 11 21 25 23 28
Acid value mgkoH/g 9.2 9.2 9.5 9.3 11 11 10 10
Solid content (%) 65 64 65 64 67 50 55 56
VOC content (g/L) 68 65 60 50 77 78 78 70
Resistance to Huang effect Δ E 1.5 1.0 0.5 1.3 3.6 4.1 4.0 3.7
Brushing surface (m2/kg) 13 16 12 14 10 8 7 6
Transparency (%) 91% 89% 90% 89% 77% 79% 76% 72%
Blush resistance (%) 88% 86% 90% 88% 81% 80% 77% 79%
Comparative example 2 compared with Example 4, comparative example 2 use unmodified white carbon black component, cause comparative example 2 viscosity and resistance to brush Area, transparency are decreased obviously, and the low easy sagging of viscosity, lead to uneven surface；Comparative example 3 compared with Example 4, does not use Modified white carbon black component, the viscosity of comparative example 3 and resistance to brush finish product, transparency overall effect are all not so good as embodiment 4.
It can be seen from Table 1 that viscosity, fineness in multi-functional dumb light cold coating sample produced by the present invention, VOC contain Amount, solid content, acid value, hydroxyl value, resistance to yellow effect, gloss indices fully meet industrial needs, meet GB/T23999- 2009 requirement for basic performance, while being better than comparative example 1-4, hardness scratch resistant effect is obvious, and curing rate is fast, filling Property is good；Applied widely, cost performance is high；Resistance to Huang effect improves 10%-25%, brushes area and improves 2%-5%, and solid content reduces, The richness of dumb light resin improves, it is preferred that the transparency of dumb light resin is improved significantly.
It is merely a preferred embodiment of the present invention, is not intended to restrict the invention, although referring to aforementioned implementation described in upper Invention is explained in detail for example, for those skilled in the art, still can be to foregoing embodiments Documented technical solution is modified or equivalent replacement of some of the technical features.It is all in spirit of the invention Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.

Claims (10)

1. a kind of multi-functional dumb light resin, which is characterized in that be grouped as by the group of following parts by weight: 60-80 parts of resin, delustring 10-30 parts of agent, 2-5 parts of dispersing agent, 20-40 parts of butyl ester compositions, wherein delustering agent is by 5-16 parts of wax emulsions of parts by weight, parts by weight 3- 2-8 parts of 6 parts of metallic soaps, parts by weight modified white carbon black compositions.
2. a kind of multi-functional dumb light resin according to claim 1, which is characterized in that used in the modified white carbon black Raw material white carbon black is fumed silica M-5 white carbon black, modified white carbon black purity 99.5-99.8%, specific surface area are as follows: 110- 150m2/ g, partial size are as follows: 7-40nm.
3. a kind of multi-functional dumb light resin according to claim 1, which is characterized in that the wax emulsion is aqueous poly- second Alkene wax emulsion.
4. a kind of multi-functional dumb light resin according to claim 1, which is characterized in that metallic soap is zinc stearate, tristearin One or more of sour calcium or odium stearate.
5. a kind of multi-functional dumb light resin according to claim 1, which is characterized in that the dispersing agent be BH616, At least one of DP983, BYKP-105 and Disper710.
6. a kind of multi-functional dumb light resin according to claim 1, which is characterized in that the resin is epoxy group acrylic acid The mass ratio of the mixture of resin and Hydroxylated acrylic resin, epoxy group acrylic resin and Hydroxylated acrylic resin is 1:1.
7. a kind of preparation method of multi-functional dumb light resin as claimed in claim 6, which is characterized in that the preparation of modified white carbon black Method is as follows:
1. score meter by weight crushes 100 parts of white carbon blacks, sieving obtains sieving, and sieving is molten with sodium tripolyphosphate 200-300 parts of liquid are mixed, and 1-2h is impregnated, and filtering obtains filter residue, filter residue washed with ferroso-ferric oxide, in temperature 100-120 It is dried at DEG C, fine powder is ground into after drying；
2. taking 3-10 parts of mutual-amido two polyaniline, 3-10 parts of nylon powder, 10-30 parts of initiator, 10-30 parts of addition reactions of polyethylene glycol Kettle is mixed, magnetic agitation 1h；
3. reaction kettle, which is added, in white carbon black obtains mixture, 99% nitrogen is injected, keeping the pressure of reaction kettle is 2.1-4Kg/cm2, temperature Degree is 500-1400 DEG C, is reacted 120 minutes, and resulting material out is put into a centrifuge and is centrifuged, centrifugation object is obtained；
4. by step, 3. for resulting centrifugation object through ultrasonic wave and microwave combined processing, ultrasonic technology parameter is frequency 20- 100KHz, 100-2000 watts of power；Microwave technology parameters frequency be 880-2500MHz, 300-1500 watts of power, Combined Treatment Time is 10-150 minutes, controls temperature at 50-70 DEG C；
5. by step, 4. resulting product is mixed with 30-50 parts of titanate coupling agents at a temperature of 30-60 DEG C and is coupled, later Refilter, wash, 600-900 DEG C calcining 2-6 hours, obtain described in modified white carbon black.
8. a kind of preparation method of multi-functional dumb light resin according to claim 7, it is characterised in that initiator is hydrogen mistake Oxide, dialkyl, diacyl peroxides any one.
9. a kind of preparation method of multi-functional dumb light resin described in -8 according to claim 1, which is characterized in that multi-functional dumb light Resin the preparation method is as follows:
1. the preparation of delustering agent: after wax emulsion is mixed evenly with metallic soap, being sprayed at modified white carbon black in spraying form Surface and mixed；
2. the delustering agent at room temperature, 1. step prepared is added in separating apparatus, revolving speed is adjusted to 400r/min, stirring Under, resin is added, revolving speed is adjusted to 1200r/min, after high speed dispersion 30min, it is stand-by to obtain homogeneous viscous fluid A；
3. being slowly added in dispersing agent under stirring, revolving speed is adjusted to 800r/min, 30min is stirred, obtains homogeneous solution B；
4. being slowly added to butyl ester in separating apparatus, revolving speed is adjusted to 400r/min, it is resulting that step (3) are added under stirring Even liquid B, is adjusted to 1200r/min for mixing speed after the completion of charging, continues to stir 20min, after test traditional performance is qualified, i.e., Dumb light resin is made.
10. a kind of application of the multi-functional dumb light resin described in claim 1-9 in paint of coating: it is characterized by: more function Energy dumb light resin is to add and stir evenly in 5-40 parts of addition paint of coating with parts by weight, is suitable for woodcare paint class.
CN201810766753.1A 2018-07-13 2018-07-13 The preparation method of multi-functional dumb light resin and its application in paint of coating Pending CN108948972A (en)

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